1、Designation: D 97 09Designation: 15/95An American National StandardStandard Test Method forPour Point of Petroleum Products1This standard is issued under the fixed designation D 97; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, t
2、he year of last revision.Anumber in parentheses indicates the year of last reapproval.Asuperscriptepsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 This test method covers and i
3、s intended for use on anypetroleum product.2A procedure suitable for black specimens,cylinder stock, and nondistillate fuel oil is described in 8.8.Thecloud point procedure formerly part of this test method nowappears as Test Method D 2500.1.2 Currently there is no ASTM test method for automatedTest
4、 Method D 97 pour point measurements.1.3 Several ASTM test methods offering alternative proce-dures for determining pour points using automatic apparatusare available. None of them share the same designation numberas Test Method D 97. When an automatic instrument is used,the ASTM test method designa
5、tion number specific to thetechnique shall be reported with the results. A procedure fortesting the pour point of crude oils is described in Test MethodD 5853.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 This standard
6、 does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM
7、Standards:3D117 Guide for Sampling, Test Methods, and Specifica-tions for Electrical Insulating Oils of Petroleum OriginD 396 Specification for Fuel OilsD 2500 Test Method for Cloud Point of Petroleum ProductsD 5853 Test Method for Pour Point of Crude OilsD 6300 Practice for Determination of Precisi
8、on and BiasData for Use in Test Methods for Petroleum Products andLubricantsE1 Specification for ASTM Liquid-in-Glass Thermometers2.2 Energy Institute Standards:Specifications for IP Standard Thermometers43. Terminology3.1 Definitions:3.1.1 black oil, nlubricant containing asphaltic materials.Black
9、oils are used in heavy-duty equipment applications, suchas mining and quarrying, where extra adhesiveness is desired.3.1.2 cylinder stock, nlubricant for independently lubri-cated engine cylinders, such as those of steam engines and aircompressors. Cylinder stock are also used for lubrication ofvalv
10、es and other elements in the cylinder area.3.1.3 pour point, nin petroleum products, the lowesttemperature at which movement of the test specimen isobserved under prescribed conditions of test.3.1.4 residual fuel, na liquid fuel containing bottomsremaining from crude distillation or thermal cracking
11、; some-times referred to as heavy fuel oil.3.1.4.1 DiscussionResidual fuels comprise Grades 4, 5,and 6 fuel oils, as defined in Specification D 396.4. Summary of Test Method4.1 After preliminary heating, the sample is cooled at aspecified rate and examined at intervals of 3C for flowcharacteristics.
12、 The lowest temperature at which movement ofthe specimen is observed is recorded as the pour point.5. Significance and Use5.1 The pour point of a petroleum specimen is an index ofthe lowest temperature of its utility for certain applications.1This test method is under the jurisdiction of ASTM Commit
13、tee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.07 on Flow Properties.Current edition approved April 15, 2009. Published April 2009. Originallyapproved in 1927, replacing D 47. Last previous edition approved in 2008 asD 9708.In the IP, this test method
14、 is under the jurisdiction of the StandardizationCommittee. This test method was adopted as a joint ASTM-IP Standard in 1965.2Statements defining this test and its significance when applied to electricalinsulating oils of mineral origin will be found in Guide D117.3For referenced ASTM standards, vis
15、it the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.4Methods forAnalysis and Testing, IP Standards for Petroleum and its Products,Part I, Vol 2.1*A
16、Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6. Apparatus6.1 Test Jar, cylindrical, of clear glass, flat bottom, 33.2 to34.8-mm outside diameter, and 115 to 125 mm in h
17、eight. Theinside diameter of the jar can range from 30.0 to 32.4 mm,within the constraint that the wall thickness be no greater than1.6 mm. The jar shall have a line to indicate a sample height 546 3 mm above the inside bottom. See Fig. 1.6.2 Thermometers, having the following ranges and con-forming
18、 to the requirements prescribed in Specification E1forthermometers:Temperature ThermometerNumberThermometer Range ASTM IPHigh cloud and pour 38 to +50C 5C 1CLow cloud and pour 80 to +20C 6C 2CMelting point +32 to +127C 61C 63C6.2.1 Since separation of liquid column thermometers occa-sionally occurs
19、and may escape detection, thermometersshould be checked immediately prior to the test and used onlyif they prove accurate within 61C (for example ice point).6.3 Cork, to fit the test jar, bored centrally for the testthermometer.6.4 Jacket, watertight, cylindrical, metal, flat-bottomed, 1156 3-mm dep
20、th, with inside diameter of 44.2 to 45.8 mm. Itshall be supported in a vertical position in the cooling bath (see6.7) so that not more than 25 mm projects out of the coolingmedium, and shall be capable of being cleaned.6.5 Disk, cork or felt, 6 mm thick to fit loosely inside thejacket.6.6 Gasket, to
21、 fit snugly around the outside of the test jarand loosely inside the jacket. The gasket may be made ofrubber, leather, or other material that is elastic enough to clingto the test jar and hard enough to hold its shape. Its purpose isto prevent the test jar from touching the jacket.6.7 Bath or Baths,
22、 maintained at prescribed temperatureswith a firm support to hold the jacket vertical. The requiredbath temperatures may be obtained by refrigeration if avail-able, otherwise by suitable cooling mixtures. Cooling mixturescommonly used for bath temperatures down to those shown areas follows:Bath Temp
23、era-tureIce and water 0 6 1.5CCrushed ice and sodium chloride crystals, or acetone orpetroleum naphtha (see Section 7) with solid carbon dioxideadded to give the desired temperature18 6 1.5CAcetone or petroleum naphtha (see Section 7) with solidcarbon dioxide added to give the desired temperature33
24、6 1.5CAcetone or petroleum naphtha (see Section 7) with solidcarbon dioxide added to give the desired temperature51 6 1.5CAcetone or petroleum naphtha (see Section 7) with solidcarbon dioxide added to give the desired temperature69 6 1.5C7. Reagents and Materials7.1 The following solvents of technic
25、al grade are appropri-ate for low-temperature bath media.7.1.1 Acetone,(WarningExtremely flammable).7.1.2 Alcohol, Ethanol (WarningFlammable).7.1.3 Alcohol, Methanol (WarningFlammable. Vaporharmful).NOTEDimensions are in millimetres (not to scale).FIG. 1 Apparatus for Pour Point TestD970927.1.4 Petr
26、oleum Naphtha,(WarningCombustible. Vaporharmful).7.1.5 Solid Carbon Dioxide,(WarningExtremely cold78.5C).8. Procedure8.1 Pour the specimen into the test jar to the level mark.When necessary, heat the specimen in a bath until it is justsufficiently fluid to pour into the test jar.NOTE 1It is known th
27、at some materials, when heated to a temperaturehigher than 45C during the preceding 24 h, do not yield the same pourpoint results as when they are kept at room temperature for 24 h prior totesting. Examples of materials which are known to show sensitivity tothermal history are residual fuels, black
28、oils, and cylinder stocks.8.1.1 Samples of residual fuels, black oils, and cylinderstocks which have been heated to a temperature higher than45C during the preceding 24 h, or when the thermal history ofthese sample types is not known, shall be kept at roomtemperature for 24 h before testing. Samples
29、 which are knownby the operator not to be sensitive to thermal history need notbe kept at room temperature for 24 h before testing.8.1.2 Experimental evidence supporting elimination of the24-h waiting period for some sample types is contained in aresearch report.58.2 Close the test jar with the cork
30、 carrying the high-pourthermometer (5.2). In the case of pour points above 36C, usea higher range thermometer such as IP 63C or ASTM 61C.Adjust the position of the cork and thermometer so the cork fitstightly, the thermometer and the jar are coaxial, and thethermometer bulb is immersed so the beginn
31、ing of the capillaryis 3 mm below the surface of the specimen.8.3 For the measurement of pour point, subject the speci-men in the test jar to the following preliminary treatment:8.3.1 Specimens Having Pour Points Above 33CHeatthe specimen without stirring to 9C above the expected pourpoint, but to a
32、t least 45C, in a bath maintained at 12C abovethe expected pour point, but at least 48C. Transfer the test jarto a bath maintained at 24 6 1.5C and commence observa-tions for pour point. When using a liquid bath, ensure that theliquid level is between the fill mark on the test jar and the topof the
33、test jar.8.3.2 Specimens Having Pour Points of 33C andBelowHeat the specimen without stirring to at least 45C ina bath maintained at 48 6 1.5C. Transfer the test jar to a bathmaintained at 24 6 1.5C. When using a liquid bath, ensurethat the liquid level is between the fill mark on the test jar andth
34、e top of the test jar. When the specimen temperature reaches27C, remove the high cloud and pour thermometer, and placethe low cloud and pour thermometer in position. Transfer thetest jar to the cooling bath (see 8.6.1).8.4 See that the disk, gasket, and the inside of the jacket areclean and dry. Pla
35、ce the disk in the bottom of the jacket. Placethe gasket around the test jar, 25 mm from the bottom. Insertthe test jar in the jacket. Never place a jar directly into thecooling medium.8.5 After the specimen has cooled to allow the formation ofparaffin wax crystals, take great care not to disturb th
36、e mass ofspecimen nor permit the thermometer to shift in the specimen;any disturbance of the spongy network of wax crystals willlead to low and erroneous results.8.6 Pour points are expressed in integers that are positive ornegative multiples of 3C. Begin to examine the appearance ofthe specimen whe
37、n the temperature of the specimen is 9Cabove the expected pour point (estimated as a multiple of 3C).At each test thermometer reading that is a multiple of 3Cbelow the starting temperature remove the test jar from thejacket. To remove condensed moisture that limits visibilitywipe the surface with a
38、clean cloth moistened in alcohol(ethanol or methanol). Tilt the jar just enough to ascertainwhether there is a movement of the specimen in the test jar. Ifmovement of specimen in the test jar is noted, then replace thetest jar immediately in the jacket and repeat a test for flow atthe next temperatu
39、re, 3C lower. Typically, the completeoperation of removal, wiping, and replacement shall requirenot more than 3 s.8.6.1 If the specimen has not ceased to flow when itstemperature has reached 27C, transfer the test jar to a jacket ina cooling bath maintained at 0 6 1.5C. As the specimencontinues to g
40、et colder, transfer the test jar to a jacket in thenext lower temperature cooling bath in accordance with Table1.8.6.2 If the specimen in the jar does not show movementwhen tilted, hold the jar in a horizontal position for 5 s, asnoted by an accurate timing device, and observe the specimencarefully.
41、 If the specimen shows any signs of movement before5 s has passed, replace the test jar immediately in the jacket andrepeat a test for flow at the next temperature, 3C lower.8.7 Continue in this manner until a point is reached at whichthe specimen shows no movement when the test jar is held ina hori
42、zontal position for 5 s. Record the observed reading ofthe test thermometer.8.8 For black specimen, cylinder stock, and nondistillatefuel specimen, the result obtained by the procedure describedin 8.1 through 8.7 is the upper (maximum) pour point. Ifrequired, determine the lower (minimum) pour point
43、 by heat-ing the sample while stirring, to 105C, pouring it into the jar,and determining the pour point as described in 8.4 through 8.7.8.9 Some specifications allow for a pass/fail test or havepour point limits at temperatures not divisible by 3C. In thesecases, it is acceptable practice to conduct
44、 the pour pointmeasurement according to the following schedule: Begin toexamine the appearance of the specimen when the temperatureof the specimen is 9C above the specification pour point.Continue observations at 3C intervals as described in 8.6 and5Supporting data have been filed at ASTM Internatio
45、nal Headquarters and maybe obtained by requesting Research Report RR: D021377.TABLE 1 Bath and Sample Temperature RangesBath Bath TemperatureSetting, CSample TemperatureRange, C106 1.5 Start to 92-186 1.5 9 to -63-36 1.5 -6to-244-56 1.5 -24 to -425-96 1.5 -42 to -60D970938.7 until the specification
46、temperature is reached. Report thesample as passing or failing the specification limit.9. Calculation and Report9.1 Add 3C to the temperature recorded in 8.7 and reportthe result as the Pour Point, ASTM D 97. For black oil, and soforth, add 3C to the temperature recorded in 8.7 and report theresult
47、as Upper Pour Point, ASTM D 97, or Lower Pour Point,ASTM D 97, as required.10. Precision and Bias10.1 PrecisionThe precision of this test method as deter-mined by the statistical examination of the interlaboratory testresults is as follows:10.1.1 Lubricating Oil6:10.1.1.1 RepeatabilityThe difference
48、 between successivetest results, obtained by the same operator using the sameapparatus under constant operating conditions on identical testmaterial would, in the long run, in the normal and correctoperation of this test method, exceed 6C only in one case intwenty. Differences greater than this shou
49、ld be consideredsuspect.10.1.1.2 ReproducibilityThe difference between twosingle and independent test results, obtained by differentoperators working in different laboratories on identical testmaterial would, in the long run, in the normal and correctoperation of this test method, exceed 9C only in one case intwenty. Differences greater than this should be consideredsuspect.10.1.1.3 The precision statements6were derived from a1998 interlaboratory test program using Practice D 6300.Participants analyzed five sets of
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